顶空气相色谱法测定西维来司钠中的残留溶剂  

Determination of Residual Solvents in Sivelestat Sodium by Head-Space Gas Chromatography

作　　者：刘冬[1] 战寒秋[2] 王茜[1] 金笃嘉[1] 冯文华[1] 兰培[1] 

机构地区：[1]中国医学科学院药物研究所,北京100050 [2]北京地坛医院,北京100015

出　　处：《中国药品标准》2010年第3期199-202,共4页Drug Standards of China

摘　　要：目的:建立了测定西维来司钠中甲醇、正己烷、乙酸乙酯、四氢呋喃、甲苯、吡啶、N,N-二甲基甲酰胺残留有机溶剂含量的顶空气相色谱法。方法:采用顶空气相色谱法,FID检测器,以二甲基亚砜为溶媒,乙醇为内标,顶空预热温度为85℃,预热时间为30min,进样口温度为180℃,检测器温度为250℃,以氮气为载气,在CIPSIL5CB的60m×0.32mm.i.d,膜厚为1μm的交联毛细管柱上,应用程序升温,实现了各组份的基线分离。结果:在甲醇、正己烷、乙酸乙酯、四氢呋喃、甲苯、吡啶、N,N-二甲基甲酰胺各自对应的浓度范围内,线性关系良好;各组分最低检测限分别为1.0,0.1,0.8,1.0,0.8,10,100mg·L-1。加样回收率(n=5)分别为97.8%(RSD=0.82%)、96.4%(RSD=1.1%)、98.1%(RSD=0.93%)、96.7%(RSD=1.8%)、101.5%(RSD=1.3%)、96.3%(RSD=1.9%)、95.2%(RSD=2.4%),精密度较好。结论:经方法学验证,该方法灵敏、准确、可靠,适用于西维来司钠中甲醇、正己烷、乙酸乙酯、四氢呋喃、甲苯、吡啶、N,N-二甲基甲酰胺等残留溶剂的测定。Objective ：This paper reports a GC method for determination of methanol, hexane, ethyl acetate, tetrahydrofuran , methyl benzene, pyridine and dimethyl formamide in Sivelestat Sodium . Method：The analytical column was CP SIL 5CB （60 mm ×0. 32 mm,1.0 μm）. The injector temperature was 180 ℃, and the detector temperature was 250 ~C. The column temperature was pro- grammed raised . The carrier gas was nitrogen, and the solvent was dimethyl sulfoxide. Results： The standard curves were linear for methanol, hexane, ethyl acetate, tetrahydrofuran , methyl benzene, pyridine and dimethyl formamide in the range of each consistency. The average recoveries （n =5） were 97.8% （ RSD =0. 82% ） for methanol, 96.4% （ RSD = 1.1% ） for hexanc, 98. 1% （ RSD = 0. 93% ） for ethyl acetate,96. 7% （RSD = 1.8% ） for tetrahydrofuran ,101.5% （RSD = 1.3% ） for methyl benzene, 96. 3% （RSD = 1.9% ） for pyfidine and 95.2% （ RSD = 2. 4% ） for dimethy formamidc respectively. Conclusion： This method is simple, rapid and precise.

关 键 词：顶空气相色谱法 西维来司钠 残留溶剂测定 

分 类 号：R123.1[医药卫生—环境卫生学]